CN106920617B - High-performance Ne-Fe-B rare earth permanent-magnetic material and preparation method thereof - Google Patents

High-performance Ne-Fe-B rare earth permanent-magnetic material and preparation method thereof Download PDF

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CN106920617B
CN106920617B CN201710170758.3A CN201710170758A CN106920617B CN 106920617 B CN106920617 B CN 106920617B CN 201710170758 A CN201710170758 A CN 201710170758A CN 106920617 B CN106920617 B CN 106920617B
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furnace
pressure
heat preservation
rare earth
sintering
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CN106920617A (en
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李军
刘颖
赵伟
向前
汤丹
黄建昕
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Sichuan University
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
    • H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
    • H01F1/047—Alloys characterised by their composition
    • H01F1/053—Alloys characterised by their composition containing rare earth metals
    • H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
    • H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/02—Compacting only
    • B22F3/04—Compacting only by applying fluid pressure, e.g. by cold isostatic pressing [CIP]
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12—Both compacting and sintering
    • B22F3/16—Both compacting and sintering in successive or repeated steps
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/74—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
    • C21D1/773—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material under reduced pressure or vacuum
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • C21D9/0068—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for particular articles not mentioned below
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/005—Ferrous alloys, e.g. steel alloys containing rare earths, i.e. Sc, Y, Lanthanides
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/10—Ferrous alloys, e.g. steel alloys containing cobalt
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/12—Ferrous alloys, e.g. steel alloys containing tungsten, tantalum, molybdenum, vanadium, or niobium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/16—Ferrous alloys, e.g. steel alloys containing copper
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
    • H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
    • H01F1/047—Alloys characterised by their composition
    • H01F1/053—Alloys characterised by their composition containing rare earth metals
    • H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
    • H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
    • H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
    • H01F1/0576—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together pressed, e.g. hot working
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
    • H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
    • H01F1/047—Alloys characterised by their composition
    • H01F1/053—Alloys characterised by their composition containing rare earth metals
    • H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
    • H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
    • H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
    • H01F1/0577—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together sintered

Abstract

A kind of preparation method of high-performance Ne-Fe-B rare earth permanent-magnetic material: (1) ingredient；(2) founding；(3) magnetic powder is prepared；(4) pressing under magnetic field green compact are prepared；(5) isostatic cool pressing；(6) isostatic cool pressing green compact obtained by step (5) are put into low-pressure sintering furnace by low pressure sintering, when being evacuated to pressure≤1 × 10 in furnace‑2It is started to warm up when Pa, when being warming up to 900~1000 DEG C of 0.5~1.0h of heat preservation, vacuum pumping is kept in above-mentioned heating and insulating process, stop vacuumizing after heat preservation, the temperature in furnace is continued at 900~1000 DEG C and is passed through pressure in high purity inert gas to furnace to be that 0.5~4MPa heat-insulation pressure keeping is sintered 5~30min, stops keeping the temperature and being passed through room temperature high purity inert gas after sintering being cooled to room temperature to obtain sintered magnet；(7) two-stage is heat-treated.The above method can obtain the Nd-Fe-B rare earth permanent magnetic material that comprehensive magnetic can be excellent, and reduce cost.

Description

High-performance Ne-Fe-B rare earth permanent-magnetic material and preparation method thereof
Technical field
The invention belongs to rare-earth permanent-magnet material technical field, in particular to a kind of method for preparing rare earth permanent-magnetic material.
Background technique
In recent years, Sintered NdFeB magnet is low in wind-power electricity generation, hybrid vehicle/pure electric automobile and energy saving household electrical appliances etc. Carbon is widely used in economic field, according to the needs of application, double high magnetic characteristics magnet (high energy products (BH)maxAnd height Intrinsic coercivity Hcj) and reduce production cost as the main target developed.Therefore, how under least cost to obtain magnet Higher comprehensive magnetic can become current urgent problem.The comprehensive magnetic of Sintered NdFeB magnet can main influence because Element is magnet consistency, grain size, distribution of intergranular phase etc..
Traditional vacuum sintering method is usually sintered by improving in sintering step to improve the consistency of neodymium iron boron magnetic body Temperature (is higher than 1040 DEG C), extends sintering time (3 hours or more) Lai Shixian.But with the raising or/and sintering of sintering temperature The extension of time, Nd2Fe14B crystal grain is inevitably grown up, and is easily caused the uneven distribution of coarse grains and intergranular phase, is led The magnet degree of orientation is caused to be deteriorated, coercivity decline, maximum magnetic energy product decline.
The patent application of Publication No. CN103123843A discloses that " a kind of fine grain anisotropy densification neodymium iron boron is forever The preparation method of magnet ", this method obtain being pre-sintered magnet blank by using low temperature presintering knot technique, then will be pre-sintered magnetic Chaeta base carries out hot-pressing densification, then carries out the sintered NdFeB magnetic that tempering obtains having both fine grain and high compactness Body.It is carried out in vacuum sintering furnace and soaking time is longer due to being pre-sintered, hot pressed sintering is grasped using in vacuum hotpressing stove Make relatively complicated, cost increase, and magnet oxidation is not easy to control；Since edge is pre-sintered magnet in hot pressed sintering densification process Blank differently- oriented directivity (axial direction) is exerted pressure very greatly, thus magnetic powder easily occurs to slide or rotate, and causes to be also easy to produce deformation, destroys magnetic Powder orientation, while hot pressing die is required also higher.
Summary of the invention
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to provide a kind of Nd-Fe-B rare earth permanent magnetic material preparation side Method, to obtain the comprehensive magnetic excellent Nd-Fe-B rare earth permanent magnetic material of energy and reduce cost.
The preparation method of high-performance Ne-Fe-B rare earth permanent-magnetic material of the present invention, processing step are as follows:
(1) ingredient
According to the component of following rare earth permanent-magnetic material and the mass percentage progress ingredient of each component: RE 27%~ 34.5%, Fe 61.5%~71%, B 0.9%~1.1%, Tm 0.1%~7%；The RE is in Nd and Pr, Ce, La At least one, the Tm are at least one of Co, Cu, Al, Ga, Nb；
(2) founding
The raw material prepared in step (1) progress founding is obtained into alloy casting piece；
(3) magnetic powder is prepared
The alloy casting piece that step (2) obtains is subjected to suction hydrogen-Dehydroepiandrosterone derivative, obtains the alloy that partial size is 10 μm~300 μm The rough and torn broken particle of gained alloy is carried out airflow milling under inert gas protection and is crushed by rough and torn broken particle, and obtaining average grain diameter is 3 μm~5 μm of mixing magnetic powder；
(4) pressing under magnetic field green compact are prepared
Antioxidant and lubricant are added into mixing magnetic powder obtained by step (3) and is uniformly mixed and forms blank, then will In blank embedded type chamber, the oriented moulding in magnetic field, obtains pressing under magnetic field green compact under inert gas protection；
(5) isostatic cool pressing
Pressing under magnetic field green compact obtained by step (4) are subjected to isostatic cool pressing, the pressure of isostatic cool pressing be 120MPa~320MPa, Time is 10s~300s, and isostatic cool pressing green compact are obtained after release；
(6) low pressure sintering
Isostatic cool pressing green compact obtained by step (5) are put into low-pressure sintering furnace and close low-pressure sintering furnace and are vacuumized, When being evacuated to pressure≤1 × 10 in furnace-2It is started to warm up when Pa, when being warming up to 900 DEG C~1000 DEG C heat preservation 0.5h~1.0h, on It states and keeps vacuum pumping in heating and insulating process, stop vacuumizing after heat preservation, continue to the temperature in furnace 900 DEG C~1000 DEG C and to be passed through in high purity inert gas to furnace pressure be that 0.5MPa~4MPa heat-insulation pressure keeping is sintered 5min~30min, Stop keeping the temperature and being passed through room temperature high purity inert gas after sintering being cooled to room temperature to obtain sintered magnet；
(7) two-stage is heat-treated
Sintered magnet obtained by step (6) is heat-treated in low-pressure sintering furnace, operation is: discharge inert gas is laggard Row vacuumizes, when being evacuated to pressure≤1 × 10 in furnace-2Started to warm up when Pa, be warming up to 800 DEG C~950 DEG C heat preservation 0.5h~ 4h, furnace cooling is to room temperature after heat preservation, then is warming up to 460 DEG C~600 DEG C heat preservation 1h~6h, and with furnace after heat preservation Room temperature is cooled to get to rare earth permanent-magnetic material, vacuum pumping is kept during above-mentioned heating, heat preservation and furnace cooling.
The preparation method of above-mentioned high-performance Ne-Fe-B rare earth permanent-magnetic material, the high purity inert gas be purity >= 99.999% nitrogen or argon gas.
The preparation method of above-mentioned high-performance Ne-Fe-B rare earth permanent-magnetic material, antioxidant and lubrication described in step (4) The total addition level of agent is mix magnetic powder quality 0.05%~0.5%, and the mass ratio of antioxidant and lubricant is 1:1；It is formed The magnetic field strength of pressing under magnetic field green compact is 1.5T~3T, and briquetting pressure is 40MPa~100MPa.Antioxidant is commercially available neodymium iron boron Special antioxidant, domestic You Duo company production, such as the happy holy new material research institute in Tianjin, Hangzhou Yadong new material are limited Company, Taiyuan Jia Ci Co., Ltd, Beijing Jun Cefeng development in science and technology Co., Ltd etc.；Lubricant can be oleic acid, stearic acid, hard Resin acid zinc etc., the present invention select zinc stearate.
The present invention also provides the high-performance Ne-Fe-B rare earth permanent-magnetic materials of above method preparation.
Compared with prior art, the invention has the following advantages:
1. since the method for the invention carries out low pressure sintering and heat treatment using the same sintering furnace, thus not only can letter Change operation, and can avoid the oxidation that magnet is easily led to when sintering furnace is converted.
2. since isostatic cool pressing green compact are carried out 0.5h~1.0h's at 900 DEG C~1000 DEG C first by the method for the invention Vacuum heat-preserving, thus be conducive to the generation and homogenization flowing of liquid phase, blank is after liquid-phase sintering is sufficiently shunk, and big hole is Eliminated, then stop vacuumizing be passed through high-purity gas apply pressure carried out at 900 DEG C~1000 DEG C, 0.5~4Mpa it is low in short-term Pressure sintering is conducive to eliminate the intracorporal microscopic pores of magnetic, improves magnet consistency, and crystal grain is avoided to grow up, thus can get comprehensive Close the Nd-Fe-B rare earth permanent magnetic material having excellent magnetic characteristics.
3. since the temperature of the method for the invention low pressure sintering is lower, and being to be applied by being passed through high-purity gas to green body Pressure, thus magnet is not easy to deviate original orientation in low-temperature short-time densification process, maintains the higher degree of orientation, has Conducive to the raising of comprehensive magnetic energy.
4. when due to using the lower temperature of same sintering furnace progress low pressure sintering and heat treatment and low pressure sintering, sintering Between it is short, thus can be energy saving, reduce production cost.
5. since the method for the invention sintering temperature is lower, and there are gas pressures outside blank when being sintered, thus Rare earth metal is not easy volatilizing loss, and the retention of rare earth element can be improved.
Specific embodiment
High-performance Ne-Fe-B rare earth permanent-magnetic material of the present invention and preparation method thereof is done into one by the following examples Walk explanation.
In following embodiment, the NdFeB rear-earth is indicated in the chemical formula of prepared Nd-Fe-B rare earth permanent magnetic material forever The component of magnetic material and the mass percentage of each component, for example, chemical formula 27.17Nd-70.59Fe-1.02B-0.72Al- The mass percentage of component and each component that 0.5Cu is indicated is as follows: Nd 27.17%, Fe 70.59%, B 1.02%, Al is 0.72%, Cu 0.5%.
Embodiment 1
The present embodiment prepares 27.17Nd-70.59Fe-1.02B-0.72Al-0.5Cu rare earth permanent-magnetic material, and processing step is such as Under:
(1) ingredient
According to the chemical formula ingredient of above-mentioned rare earth permanent-magnetic material, and by the oxide on raw metal surface and to be mingled with removing dry Only；
(2) founding
The raw material that step (1) prepares is put into vacuum induction melting furnace, melting under the conditions of high-purity argon gas will close after melting Golden liquid casting on-line velocity is that the rapid hardening that average thickness is 0.25mm is obtained after being quickly cooled down on the water-cooled copper roller of 3m/s Alloy casting piece；
(3) magnetic powder is prepared
Alloy casting piece that step (2) obtains merging rotation hydrogen blasting furnace is subjected to suction hydrogen-Dehydroepiandrosterone derivative, obtain partial size be 10~ The rough and torn broken particle of gained alloy is carried out airflow milling under nitrogen protection and is crushed, is averaged by the rough and torn broken particle of 300 μm of alloy The mixing magnetic powder that partial size is 3 μm；
(4) pressing under magnetic field green compact are prepared
The antioxidant and lubricant (oxygen of addition mixing magnetic powder quality 0.25wt% into mixing magnetic powder obtained by step (3) The mass ratio 1:1 of agent and lubricant), antioxidant is commercially available neodymium iron boron special antioxidant, and lubricant selects zinc stearate, It is uniformly mixed in batch mixer and forms blank, then by blank embedded type chamber, be in magnetic field strength under nitrogen protection Oriented moulding in the magnetic field of 1.8T, briquetting pressure 60MPa obtain pressing under magnetic field green compact；
(5) isostatic cool pressing
Pressing under magnetic field green compact obtained by step (4) are subjected to isostatic cool pressing, the pressure of isostatic cool pressing is 200MPa, isostatic cool pressing Time is 120s, and isostatic cool pressing green compact are obtained after release；
(6) low pressure sintering
Isostatic cool pressing green compact obtained by step (5) are put into low-pressure sintering furnace and close low-pressure sintering furnace and are vacuumized, When being evacuated to pressure≤1 × 10 in furnace-2It starts to warm up when Pa, when being warming up to 980 DEG C of heat preservation 1.0h, above-mentioned heating and kept the temperature Vacuum pumping is kept in journey, is stopped vacuumizing after heat preservation, is continued to the temperature in furnace at 980 DEG C and be passed through high-purity argon Pressure is that 2MPa heat-insulation pressure keeping is sintered 25min in gas to furnace, stops keeping the temperature and being passed through the progress of room temperature high-purity argon gas after sintering It is cooling, obtain sintered magnet；
(7) two-stage is heat-treated
Sintered magnet obtained by step (6) is heat-treated in low-pressure sintering furnace, operation is: discharge inert gas is laggard Row vacuumizes, when being evacuated to pressure≤1 × 10 in furnace-2It is started to warm up when Pa, is warming up to 920 DEG C of heat preservation 1.5h, heat preservation terminates Furnace cooling is to room temperature afterwards, then is warming up to 510 DEG C of heat preservation 4h, and furnace cooling arrives rare earth to room temperature after heat preservation Permanent-magnet material keeps vacuum pumping during above-mentioned heating, heat preservation and furnace cooling.
Comparative example 1
Step (6) is sintered using traditional vacuum, remaining step is same as Example 1.Vacuum sintering technology is 10-3~ 10-2In 1060 DEG C of heat preservation sintering 4h under Pa vacuum condition, it is passed through room temperature high-purity argon gas after sintering and is cooled down, is sintered Magnet.
The rare earth permanent-magnetic material and embodiment 1 prepared with AMT-4 magnetization characteristic automatic measuring instrument difference test comparison example 1 is made The magnetic property of the magnetic property of standby rare earth permanent-magnetic material, gained magnet is as follows:
Embodiment 2
The present embodiment prepares 29.28Nd-68.15Fe-1.02B-0.85Al-0.7Cu rare earth permanent-magnetic material, and processing step is such as Under:
(1) ingredient
According to the chemical formula ingredient of above-mentioned rare earth permanent-magnetic material, and by the oxide on raw metal surface and to be mingled with removing dry Only；
(2) founding
The raw material that step (1) prepares is put into vacuum induction melting furnace, melting under the conditions of high-purity argon gas will close after melting Golden liquid casting on-line velocity is that the rapid hardening that average thickness is 0.25mm is obtained after being quickly cooled down on the water-cooled copper roller of 3m/s Alloy casting piece；
(3) magnetic powder is prepared
Alloy casting piece that step (2) obtains merging rotation hydrogen blasting furnace is subjected to suction hydrogen-Dehydroepiandrosterone derivative, obtain partial size be 10~ The rough and torn broken particle of gained alloy is carried out airflow milling under nitrogen protection and is crushed, is averaged by the rough and torn broken particle of 300 μm of alloy The mixing magnetic powder that partial size is 3.5 μm；
(4) pressing under magnetic field green compact are prepared
Into mixing magnetic powder obtained by step (3), the antioxidant of addition mixing magnetic powder quality 0.15wt% and lubricant are (anti- Oxidant and lubricant mass ratio 1:1), antioxidant is commercially available neodymium iron boron special antioxidant, and lubricant selects zinc stearate, It is uniformly mixed in batch mixer and forms blank, then by blank embedded type chamber, be in magnetic field strength under nitrogen protection Oriented moulding in the magnetic field of 1.5T, briquetting pressure 80MPa obtain pressing under magnetic field green compact；
(5) isostatic cool pressing
Pressing under magnetic field green compact obtained by step (4) are subjected to isostatic cool pressing, the pressure of isostatic cool pressing is 150MPa, isostatic cool pressing Time is 100s, and isostatic cool pressing green compact are obtained after release；
(6) low pressure sintering
Isostatic cool pressing green compact obtained by step (5) are put into low-pressure sintering furnace and close low-pressure sintering furnace and are vacuumized, When being evacuated to pressure≤1 × 10 in furnace-2It starts to warm up when Pa, when being warming up to 980 DEG C of heat preservation 1.0h, above-mentioned heating and kept the temperature Vacuum pumping is kept in journey, is stopped vacuumizing after heat preservation, is continued to the temperature in furnace at 980 DEG C and be passed through high-purity argon Pressure is that 2MPa heat-insulation pressure keeping is sintered 25min in gas to furnace, stops keeping the temperature and being passed through the progress of room temperature high-purity argon gas after sintering It is cooling, obtain sintered magnet；
(7) two-stage is heat-treated
Sintered magnet obtained by step (6) is heat-treated in low-pressure sintering furnace, operation is: discharge inert gas is laggard Row vacuumizes, when being evacuated to pressure≤1 × 10 in furnace-2It is started to warm up when Pa, 910 DEG C of heat preservation 1h is warming up to, after heat preservation Furnace cooling is to room temperature, then is warming up to 530 DEG C of heat preservation 3h, and furnace cooling arrives rare earth forever to room temperature after heat preservation Magnetic material keeps vacuum pumping during above-mentioned heating, heat preservation and furnace cooling.
Comparative example 2
Step (6) is sintered using traditional vacuum, remaining step is same as Example 2.Vacuum sintering technology is 10-3~ 10-2In 1055 DEG C of heat preservation sintering 4h under Pa vacuum condition, it is passed through room temperature high-purity argon gas after sintering and is cooled down, is sintered Magnet.
The rare earth permanent-magnetic material and embodiment 2 prepared with AMT-4 magnetization characteristic automatic measuring instrument difference test comparison example 2 is made The magnetic property of the magnetic property of standby rare earth permanent-magnetic material, gained magnet is as follows:
Embodiment 3
The present embodiment prepares 29.82 (Nd, Pr) -62.42Fe-4.97Co-1.0B-0.83Ga-0.96Cu rare earth permanent magnet materials Material, processing step are as follows:
(1) ingredient
According to the chemical formula ingredient of above-mentioned rare earth permanent-magnetic material, and by the oxide on raw metal surface and to be mingled with removing dry Only；
(2) founding: being put into vacuum induction melting furnace for the raw material that step (1) prepares, melting under the conditions of high-purity argon gas, melts By aluminium alloy casting on-line velocity on the water-cooled copper roller of 3m/s, obtaining average thickness after being quickly cooled down is after refining The rapid hardening alloy casting piece of 0.25mm；
(3) magnetic powder is prepared
Alloy casting piece that step (2) obtains merging rotation hydrogen blasting furnace is subjected to suction hydrogen-Dehydroepiandrosterone derivative, obtain partial size be 10~ The rough and torn broken particle of gained alloy is carried out airflow milling under nitrogen protection and is crushed, is averaged by the rough and torn broken particle of 300 μm of alloy The mixing magnetic powder that partial size is 4 μm；
(4) pressing under magnetic field green compact are prepared
The antioxidant and lubricant (antioxygen of addition mixing magnetic powder quality 0.2wt% into mixing magnetic powder obtained by step (3) Agent and lubricant mass ratio 1:1), antioxidant is commercially available neodymium iron boron special antioxidant, and lubricant selects zinc stearate, Be uniformly mixed in batch mixer and form blank, then by blank embedded type chamber, under nitrogen protection in magnetic field strength be 1.8T Magnetic field in oriented moulding, briquetting pressure 70MPa obtains pressing under magnetic field green compact；
(5) isostatic cool pressing
Pressing under magnetic field green compact obtained by step (4) are subjected to isostatic cool pressing, the pressure of isostatic cool pressing is 150MPa, isostatic cool pressing Time is 100s, and isostatic cool pressing green compact are obtained after release；
(6) low pressure sintering
Isostatic cool pressing green compact obtained by step (5) are put into low-pressure sintering furnace and close low-pressure sintering furnace and are vacuumized, When being evacuated to pressure≤1 × 10 in furnace-2It is started to warm up when Pa, when being warming up to 980 DEG C of heat preservation 50min, above-mentioned heating and heat preservation Vacuum pumping is kept in the process, is stopped vacuumizing after heat preservation, is continued to the temperature in furnace at 980 DEG C and be passed through high-purity In argon gas to furnace pressure be 2MPa heat-insulation pressure keeping be sintered 15min, after sintering stop keep the temperature and be passed through room temperature high-purity argon gas into Row cooling, obtains sintered magnet；
(7) two-stage is heat-treated
Sintered magnet obtained by step (6) is heat-treated in low-pressure sintering furnace, operation is: discharge inert gas is laggard Row vacuumizes, when being evacuated to pressure≤1 × 10 in furnace-2It is started to warm up when Pa, is warming up to 900 DEG C of heat preservation 1.5h, heat preservation terminates Furnace cooling is to room temperature afterwards, then is warming up to 530 DEG C of heat preservation 4h, and furnace cooling arrives rare earth to room temperature after heat preservation Permanent-magnet material keeps vacuum pumping during above-mentioned heating, heat preservation and furnace cooling.
Comparative example 3
Step (6) is sintered using traditional vacuum, remaining step is same as Example 3.Vacuum sintering technology is 10-3~ 10-2In 1050 DEG C of heat preservation sintering 4h under Pa vacuum condition, it is passed through room temperature high-purity argon gas after sintering and is cooled down, is sintered Magnet.
The rare earth permanent-magnetic material and embodiment 3 prepared with AMT-4 magnetization characteristic automatic measuring instrument difference test comparison example 3 is made The magnetic property of the magnetic property of standby rare earth permanent-magnetic material, gained magnet is as follows:
Embodiment 4
The present embodiment prepares 29.82 (Nd, Pr) -62.42Fe-4.97Co-1.0B-0.83Ga-0.96Cu rare earth permanent magnet materials Material, processing step are as follows:
(1) ingredient
According to the chemical formula ingredient of above-mentioned rare earth permanent-magnetic material, and by the oxide on raw metal surface and to be mingled with removing dry Only；
(2) founding
The raw material that step (1) prepares is respectively put into vacuum induction melting furnace, melting under the conditions of high-purity argon gas, after melting It is on the water-cooled copper roller of 3m/s by aluminium alloy casting on-line velocity, it is 0.25mm's that average thickness is obtained after being quickly cooled down Rapid hardening alloy casting piece；
(3) magnetic powder is prepared
Alloy casting piece that step (2) obtains merging rotation hydrogen blasting furnace is subjected to suction hydrogen-Dehydroepiandrosterone derivative, obtain partial size be 10~ The rough and torn broken particle of gained alloy is carried out airflow milling under nitrogen protection and is crushed, is averaged by the rough and torn broken particle of 300 μm of alloy The mixing magnetic powder that partial size is 4 μm；
(4) pressing under magnetic field green compact are prepared
Into mixing magnetic powder obtained by step (3), the antioxidant of addition mixing magnetic powder quality 0.25wt% and lubricant are (anti- Oxidant and lubricant mass ratio 1:1), antioxidant is commercially available neodymium iron boron special antioxidant, and lubricant selects zinc stearate, It is uniformly mixed in batch mixer and forms blank, then by blank embedded type chamber, be in magnetic field strength under nitrogen protection Oriented moulding in the magnetic field of 1.8T, briquetting pressure 70MPa obtain pressing under magnetic field green compact；
(5) isostatic cool pressing
Pressing under magnetic field green compact obtained by step (4) are subjected to isostatic cool pressing, the pressure of isostatic cool pressing is 150MPa, isostatic cool pressing Time is 100s, and isostatic cool pressing green compact are obtained after release；
(6) low pressure sintering
Isostatic cool pressing green compact obtained by step (5) are put into low-pressure sintering furnace and close low-pressure sintering furnace and are vacuumized, When being evacuated to pressure≤1 × 10 in furnace-2It starts to warm up when Pa, when being warming up to 980 DEG C of heat preservation 1.0h, above-mentioned heating and kept the temperature Vacuum pumping is kept in journey, is stopped vacuumizing after heat preservation, is continued to the temperature in furnace at 980 DEG C and be passed through high-purity argon Pressure is that 2MPa heat-insulation pressure keeping is sintered 25min in gas to furnace, stops keeping the temperature and being passed through the progress of room temperature high-purity argon gas after sintering It is cooling, obtain sintered magnet；
(7) two-stage is heat-treated
Sintered magnet obtained by step (6) is heat-treated in low-pressure sintering furnace, operation is: discharge inert gas is laggard Row vacuumizes, when being evacuated to pressure≤1 × 10 in furnace-2It is started to warm up when Pa, is warming up to 900 DEG C of heat preservation 1.5h, heat preservation terminates Furnace cooling is to room temperature afterwards, then is warming up to 530 DEG C of heat preservation 4h, and furnace cooling arrives rare earth to room temperature after heat preservation Permanent-magnet material keeps vacuum pumping during above-mentioned heating, heat preservation and furnace cooling.
Comparative example 4
Step (6) is sintered using traditional vacuum, remaining step is same as Example 4.Vacuum sintering technology is 10-3~ 10-2In 1060 DEG C of heat preservation sintering 4h under Pa vacuum condition, it is passed through room temperature high-purity argon gas after sintering and is cooled down, is sintered Magnet.
The rare earth permanent-magnetic material and embodiment 4 prepared with AMT-4 magnetization characteristic automatic measuring instrument difference test comparison example 4 is made The magnetic property of the magnetic property of standby rare earth permanent-magnetic material, gained magnet is as follows:
Embodiment 5
The present embodiment prepares 23.52Nd-8.88Ce-65.41Fe-0.96B-0.63Al-0.6Cu rare earth permanent-magnetic material, work Steps are as follows for skill:
(1) ingredient
According to the chemical formula ingredient of above-mentioned rare earth permanent-magnetic material, and by the oxide on raw metal surface and to be mingled with removing dry Only；
(2) founding
The raw material that step (1) prepares is put into vacuum induction melting furnace, melting under the conditions of high-purity argon gas will close after melting Golden liquid casting on-line velocity is that the rapid hardening that average thickness is 0.25mm is obtained after being quickly cooled down on the water-cooled copper roller of 3m/s Alloy casting piece；
(3) magnetic powder is prepared
The alloy casting piece merging that step (2) obtains is rotated in hydrogen blasting furnace and carries out suction hydrogen-Dehydroepiandrosterone derivative, obtaining partial size is 10 The rough and torn broken particle of gained alloy is carried out airflow milling under nitrogen protection and is crushed, put down by the rough and torn broken particle of~300 μm of alloy The mixing magnetic powder that equal partial size is 4.5 μm；
(4) pressing under magnetic field green compact are prepared
The antioxidant and lubricant (antioxygen of addition mixing magnetic powder quality 0.2wt% into mixing magnetic powder obtained by step (3) Agent and lubricant mass ratio 1:1), antioxidant is commercially available neodymium iron boron special antioxidant, and lubricant selects zinc stearate, Be uniformly mixed in batch mixer and form blank, then by blank embedded type chamber, under nitrogen protection in magnetic field strength be 2T's Oriented moulding in magnetic field, briquetting pressure 60MPa obtain pressing under magnetic field green compact；
(5) isostatic cool pressing
Pressing under magnetic field green compact obtained by step (4) are subjected to isostatic cool pressing, the pressure of isostatic cool pressing is 200MPa, isostatic cool pressing Time is 150s, and isostatic cool pressing green compact are obtained after release；
(6) low pressure sintering
Isostatic cool pressing green compact obtained by step (5) are put into low-pressure sintering furnace and close low-pressure sintering furnace and are vacuumized, When being evacuated to pressure≤1 × 10 in furnace-2It starts to warm up when Pa, when being warming up to 975 DEG C of heat preservation 1.0h, above-mentioned heating and kept the temperature Vacuum pumping is kept in journey, is stopped vacuumizing after heat preservation, is continued to the temperature in furnace at 975 DEG C and be passed through high-purity argon Pressure is that 2MPa heat-insulation pressure keeping is sintered 25min in gas to furnace, stops keeping the temperature and being passed through the progress of room temperature high-purity argon gas after sintering It is cooling, obtain sintered magnet；
(7) two-stage is heat-treated
Sintered magnet obtained by step (6) is heat-treated in low-pressure sintering furnace, operation is: discharge inert gas is laggard Row vacuumizes, when being evacuated to pressure≤1 × 10 in furnace-2It is started to warm up when Pa, is warming up to 890 DEG C of heat preservation 1.5h, heat preservation terminates Furnace cooling is to room temperature afterwards, then is warming up to 500 DEG C of heat preservation 4h, and furnace cooling arrives rare earth to room temperature after heat preservation Permanent-magnet material keeps vacuum pumping during above-mentioned heating, heat preservation and furnace cooling.
Comparative example 5
Step (6) is sintered using traditional vacuum, remaining step is same as Example 5.Vacuum sintering technology is 10-3~ 10-2In 1055 DEG C of heat preservation sintering 4h under Pa vacuum condition, it is passed through room temperature high-purity argon gas after sintering and is cooled down, is sintered Magnet.
The rare earth permanent-magnetic material and embodiment 5 prepared with AMT-4 magnetization characteristic automatic measuring instrument difference test comparison example 5 is made The magnetic property of the magnetic property of standby rare earth permanent-magnetic material, gained magnet is as follows:
Embodiment 6
The present embodiment prepares 22.13Nd-11.84Ce-63.69Fe-0.94B-0.9Al-0.5Cu rare earth permanent-magnetic material, work Steps are as follows for skill:
(1) ingredient
According to the chemical formula ingredient of above-mentioned rare earth permanent-magnetic material, and by the oxide on raw metal surface and to be mingled with removing dry Only；
(2) founding
The raw material that step (1) prepares is put into vacuum induction melting furnace, melting under the conditions of high-purity argon gas will close after melting Golden liquid casting on-line velocity is that the rapid hardening that average thickness is 0.25mm is obtained after being quickly cooled down on the water-cooled copper roller of 3m/s Alloy casting piece；
(3) magnetic powder is prepared
Alloy casting piece that step (2) obtains merging rotation hydrogen blasting furnace is subjected to suction hydrogen-Dehydroepiandrosterone derivative, obtain partial size be 10~ The rough and torn broken particle of gained alloy is carried out airflow milling under nitrogen protection and is crushed, is averaged by the rough and torn broken particle of 300 μm of alloy The mixing magnetic powder that partial size is 4 μm；
(4) pressing under magnetic field green compact are prepared
Into mixing magnetic powder obtained by step (3), the antioxidant of addition mixing magnetic powder quality 0.25wt% and lubricant are (anti- Oxidant and lubricant mass ratio 1:1), antioxidant is commercially available neodymium iron boron special antioxidant, and lubricant selects zinc stearate, It is uniformly mixed in batch mixer and forms blank, then by blank embedded type chamber, be in magnetic field strength under nitrogen protection Oriented moulding in the magnetic field of 1.8T, briquetting pressure 60MPa obtain pressing under magnetic field green compact；
(5) isostatic cool pressing
Pressing under magnetic field green compact obtained by step (4) are subjected to isostatic cool pressing, the pressure of isostatic cool pressing is 200MPa, isostatic cool pressing Time is 100s, and isostatic cool pressing green compact are obtained after release；
(6) low pressure sintering
Isostatic cool pressing green compact obtained by step (5) are put into low-pressure sintering furnace and close low-pressure sintering furnace and are vacuumized, When being evacuated to pressure≤1 × 10 in furnace-2It is started to warm up when Pa, when being warming up to 950 DEG C of heat preservation 45min, above-mentioned heating and heat preservation Vacuum pumping is kept in the process, is stopped vacuumizing after heat preservation, is continued to the temperature in furnace at 950 DEG C and be passed through high-purity Pressure is that 2MPa heat-insulation pressure keeping is sintered 5min in argon gas to furnace, stops keeping the temperature and being passed through the progress of room temperature high-purity argon gas after sintering It is cooling, obtain sintered magnet；
(7) two-stage is heat-treated
Sintered magnet obtained by step (6) is heat-treated in low-pressure sintering furnace, operation is: discharge inert gas is laggard Row vacuumizes, when being evacuated to pressure≤1 × 10 in furnace-2It is started to warm up when Pa, 890 DEG C of heat preservation 1h is warming up to, after heat preservation Furnace cooling is to room temperature, then is warming up to 505 DEG C of heat preservation 4h, and furnace cooling arrives rare earth forever to room temperature after heat preservation Magnetic material keeps vacuum pumping during above-mentioned heating, heat preservation and furnace cooling.
Comparative example 6
Step (6) is sintered using traditional vacuum, remaining step is same as Example 6.Vacuum sintering technology is 10-3~ 10-2In 1065 DEG C of heat preservation sintering 4h under Pa vacuum condition, it is passed through room temperature high-purity argon gas after sintering and is cooled down, is sintered Magnet.
The rare earth permanent-magnetic material and embodiment 6 prepared with AMT-4 magnetization characteristic automatic measuring instrument difference test comparison example 6 is made The magnetic property of the magnetic property of standby rare earth permanent-magnetic material, gained magnet is as follows:
Embodiment 7
The present embodiment prepares 23.44 (Pr, Nd) -8.45Ce-66.21Fe-0.99B-0.91Al rare earth permanent-magnetic materials, technique Steps are as follows:
(1) ingredient
According to the chemical formula ingredient of above-mentioned rare earth permanent-magnetic material, and by the oxide on raw metal surface and to be mingled with removing dry Only；
(2) founding
The raw material that step (1) prepares is put into vacuum induction melting furnace, melting under the conditions of high-purity argon gas will close after melting Golden liquid casting on-line velocity is that the rapid hardening that average thickness is 0.25mm is obtained after being quickly cooled down on the water-cooled copper roller of 3m/s Alloy casting piece；
(3) magnetic powder is prepared
The alloy casting piece merging that step (2) obtains is rotated in hydrogen blasting furnace and carries out suction hydrogen-Dehydroepiandrosterone derivative, obtaining partial size is 10 The rough and torn broken particle of gained alloy is carried out airflow milling under nitrogen protection and is crushed, put down by the rough and torn broken particle of~300 μm of alloy The mixing magnetic powder that equal partial size is 4 μm；
(4) pressing under magnetic field green compact are prepared
Into mixing magnetic powder obtained by step (3), the antioxidant of addition mixing magnetic powder quality 0.25wt% and lubricant are (anti- Oxidant and lubricant mass ratio 1:1), antioxidant is commercially available neodymium iron boron special antioxidant, and lubricant selects zinc stearate, It is uniformly mixed in batch mixer and forms blank, then by blank embedded type chamber, be in magnetic field strength under nitrogen protection Oriented moulding in the magnetic field of 1.8T, briquetting pressure 70MPa obtain pressing under magnetic field green compact；
(5) isostatic cool pressing
Pressing under magnetic field green compact obtained by step (4) are subjected to isostatic cool pressing, the pressure of isostatic cool pressing is 180MPa, isostatic cool pressing Time is 120s, and isostatic cool pressing green compact are obtained after release；
(6) low pressure sintering
Isostatic cool pressing green compact obtained by step (5) are put into low-pressure sintering furnace and close low-pressure sintering furnace and are vacuumized, When being evacuated to pressure≤1 × 10 in furnace-2It starts to warm up when Pa, when being warming up to 970 DEG C of heat preservation 1.0h, above-mentioned heating and kept the temperature Vacuum pumping is kept in journey, is stopped vacuumizing after heat preservation, is continued to the temperature in furnace at 980 DEG C and be passed through High Purity Nitrogen In gas to furnace pressure be 4MPa heat-insulation pressure keeping be sintered 5min, after sintering stop keep the temperature and be passed through room temperature high pure nitrogen carry out it is cold But, sintered magnet is obtained；
(7) two-stage is heat-treated
Sintered magnet obtained by step (6) is heat-treated in low-pressure sintering furnace, operation is: discharge inert gas is laggard Row vacuumizes, when being evacuated to pressure≤1 × 10 in furnace-2It is started to warm up when Pa, is warming up to 905 DEG C of heat preservation 1.5h, heat preservation terminates Furnace cooling is to room temperature afterwards, then is warming up to 540 DEG C of heat preservation 4h, and furnace cooling arrives rare earth to room temperature after heat preservation Permanent-magnet material keeps vacuum pumping during above-mentioned heating, heat preservation and furnace cooling.
Comparative example 7
Step (6) is sintered using traditional vacuum, remaining step is same as Example 7.Vacuum sintering technology is 10-3~ 10-2In 1060 DEG C of heat preservation sintering 4h under Pa vacuum condition, it is passed through room temperature high-purity argon gas after sintering and is cooled down, is sintered Magnet.
The rare earth permanent-magnetic material and embodiment 7 prepared with AMT-4 magnetization characteristic automatic measuring instrument difference test comparison example 7 is made The magnetic property of the magnetic property of standby rare earth permanent-magnetic material, gained magnet is as follows:
Embodiment 8
The present embodiment prepares 20.68 (Nd, Pr) -13.08Ce-64.22Fe-0.97B-0.54Al-0.51Cu rare earth permanent magnets Material, processing step are as follows:
(1) ingredient
According to the chemical formula ingredient of above-mentioned rare earth permanent-magnetic material, and by the oxide on raw metal surface and to be mingled with removing dry Only；
(2) founding
The raw material that step (1) prepares is put into vacuum induction melting furnace, melting under the conditions of high-purity argon gas will close after melting Golden liquid casting on-line velocity is that the rapid hardening that average thickness is 0.25mm is obtained after being quickly cooled down on the water-cooled copper roller of 3m/s Alloy casting piece；
(3) magnetic powder is prepared
Alloy casting piece that step (2) obtains merging rotation hydrogen blasting furnace is subjected to suction hydrogen-Dehydroepiandrosterone derivative, obtain partial size be 10~ The rough and torn broken particle of gained alloy is carried out airflow milling under nitrogen protection and is crushed, is averaged by the rough and torn broken particle of 300 μm of alloy The mixing magnetic powder that partial size is 3.5 μm；
(4) pressing under magnetic field green compact are prepared
Into mixing magnetic powder obtained by step (3), the antioxidant of addition mixing magnetic powder quality 0.25wt% and lubricant are (anti- Oxidant and lubricant mass ratio 1:1), antioxidant is commercially available neodymium iron boron special antioxidant, and lubricant selects zinc stearate, Be uniformly mixed in batch mixer and form blank, then by blank embedded type chamber, under nitrogen protection in magnetic field strength be 2T Magnetic field in oriented moulding, briquetting pressure 60MPa obtains pressing under magnetic field green compact；
(5) isostatic cool pressing
Pressing under magnetic field green compact obtained by step (4) are subjected to isostatic cool pressing, the pressure of isostatic cool pressing is 200MPa, isostatic cool pressing Time is 100s, and isostatic cool pressing green compact are obtained after release；
(6) low pressure sintering
Isostatic cool pressing green compact obtained by step (5) are put into low-pressure sintering furnace and close low-pressure sintering furnace and are vacuumized, When being evacuated to pressure≤1 × 10 in furnace-2It is started to warm up when Pa, when being warming up to 960 DEG C of heat preservation 45min, above-mentioned heating and heat preservation Vacuum pumping is kept in the process, is stopped vacuumizing after heat preservation, is continued to the temperature in furnace at 960 DEG C and be passed through high-purity In argon gas to furnace pressure be 4MPa heat-insulation pressure keeping be sintered 25min, after sintering stop keep the temperature and be passed through room temperature high-purity argon gas into Row cooling, obtains sintered magnet；
(7) two-stage is heat-treated
Sintered magnet obtained by step (6) is heat-treated in low-pressure sintering furnace, operation is: discharge inert gas is laggard Row vacuumizes, when being evacuated to pressure≤1 × 10 in furnace-2It is started to warm up when Pa, is warming up to 880 DEG C of heat preservation 1.5h, heat preservation terminates Furnace cooling is to room temperature afterwards, then is warming up to 510 DEG C of heat preservation 4h, and furnace cooling arrives rare earth to room temperature after heat preservation Permanent-magnet material keeps vacuum pumping during above-mentioned heating, heat preservation and furnace cooling.
Comparative example 8
Step (6) is sintered using traditional vacuum, remaining step is same as Example 8.Vacuum sintering technology is 10-3~ 10-2In 1060 DEG C of heat preservation sintering 4h under Pa vacuum condition, it is passed through room temperature high-purity argon gas after sintering and is cooled down, is sintered Magnet.
The rare earth permanent-magnetic material and embodiment 8 prepared with AMT-4 magnetization characteristic automatic measuring instrument difference test comparison example 8 is made The magnetic property of the magnetic property of standby rare earth permanent-magnetic material, gained magnet is as follows:
Embodiment 9
The present embodiment prepares 23.43 (Pr, Nd) -8.88Ce-64.71Fe-0.8Co-0.96B-0.5Al-0.72Cu rare earths Permanent-magnet material, processing step are as follows:
(1) ingredient
According to the chemical formula ingredient of above-mentioned rare earth permanent-magnetic material, and by the oxide on raw metal surface and to be mingled with removing dry Only；
(2) founding
The raw material that step (1) prepares is put into vacuum induction melting furnace, melting under the conditions of high-purity argon gas will close after melting Golden liquid casting on-line velocity is that the rapid hardening that average thickness is 0.25mm is obtained after being quickly cooled down on the water-cooled copper roller of 3m/s Alloy casting piece；
(3) magnetic powder is prepared
Alloy casting piece that step (2) obtains merging rotation hydrogen blasting furnace is subjected to suction hydrogen-Dehydroepiandrosterone derivative, obtain partial size be 10~ The rough and torn broken particle of gained alloy is carried out airflow milling under nitrogen protection and is crushed, is averaged by the rough and torn broken particle of 300 μm of alloy The mixing magnetic powder that partial size is 4 μm；
(4) pressing under magnetic field green compact are prepared
The antioxidant and lubricant (antioxygen of addition mixing magnetic powder quality 0.1wt% into mixing magnetic powder obtained by step (3) Agent and lubricant mass ratio 1:1), antioxidant is commercially available neodymium iron boron special antioxidant, and lubricant selects zinc stearate, Be uniformly mixed in batch mixer and form blank, then by blank embedded type chamber, under nitrogen protection in magnetic field strength be 1.8T Magnetic field in oriented moulding, briquetting pressure 60MPa obtains pressing under magnetic field green compact；
(5) isostatic cool pressing
Pressing under magnetic field green compact obtained by step (4) are subjected to isostatic cool pressing, the pressure of isostatic cool pressing is 200MPa, isostatic cool pressing Time is 150s, and isostatic cool pressing green compact are obtained after release；
(6) low pressure sintering
Isostatic cool pressing green compact obtained by step (5) are put into low-pressure sintering furnace and close low-pressure sintering furnace and are vacuumized, When being evacuated to pressure≤1 × 10 in furnace-2It starts to warm up when Pa, when being warming up to 970 DEG C of heat preservation 1.0h, above-mentioned heating and kept the temperature Vacuum pumping is kept in journey, is stopped vacuumizing after heat preservation, is continued to the temperature in furnace at 970 DEG C and be passed through high-purity argon In gas to furnace pressure be 0.5MPa heat-insulation pressure keeping be sintered 25min, after sintering stop keep the temperature and be passed through room temperature high-purity argon gas into Row cooling, obtains sintered magnet；
(7) two-stage is heat-treated
Sintered magnet obtained by step (6) is heat-treated in low-pressure sintering furnace, operation is: discharge inert gas is laggard Row vacuumizes, when being evacuated to pressure≤1 × 10 in furnace-2It is started to warm up when Pa, is warming up to 905 DEG C of heat preservation 1.5h, heat preservation terminates Furnace cooling is to room temperature afterwards, then is warming up to 540 DEG C of heat preservation 4h, and furnace cooling arrives rare earth to room temperature after heat preservation Permanent-magnet material keeps vacuum pumping during above-mentioned heating, heat preservation and furnace cooling.
Comparative example 9
Step (6) is sintered using traditional vacuum, remaining step is same as Example 9.Vacuum sintering technology is 10-3~ 10-2In 1055 DEG C of heat preservation sintering 4h under Pa vacuum condition, it is passed through room temperature high-purity argon gas after sintering and is cooled down, is sintered Magnet.
The rare earth permanent-magnetic material and embodiment 9 prepared with AMT-4 magnetization characteristic automatic measuring instrument difference test comparison example 9 is made The magnetic property of the magnetic property of standby rare earth permanent-magnetic material, gained magnet is as follows:
Embodiment 10
The present embodiment prepares 26.44 (Pr, Nd) -8.01Ce-62.19Fe-0.92B-1.0Co-0.91Al-0.53Cu rare earths Permanent-magnet material, processing step are as follows:
(1) ingredient
According to the chemical formula ingredient of above-mentioned rare earth permanent-magnetic material, and by the oxide on raw metal surface and to be mingled with removing dry Only；
(2) founding
The raw material that step (1) prepares is put into vacuum induction melting furnace, melting under the conditions of high-purity argon gas will close after melting Golden liquid casting on-line velocity is that the rapid hardening that average thickness is 0.25mm is obtained after being quickly cooled down on the water-cooled copper roller of 3m/s Alloy casting piece；
(3) magnetic powder is prepared
Alloy casting piece that step (2) obtains merging rotation hydrogen blasting furnace is subjected to suction hydrogen-Dehydroepiandrosterone derivative, obtain partial size be 10~ The rough and torn broken particle of gained alloy is carried out airflow milling under nitrogen protection and is crushed, is averaged by the rough and torn broken particle of 300 μm of alloy The mixing magnetic powder that partial size is 3.5 μm；
(4) pressing under magnetic field green compact are prepared
The antioxidant and lubricant (antioxygen of addition mixing magnetic powder quality 0.2wt% into mixing magnetic powder obtained by step (3) Agent and lubricant mass ratio 1:1), antioxidant is commercially available neodymium iron boron special antioxidant, and lubricant selects zinc stearate, Be uniformly mixed in batch mixer and form blank, then by blank embedded type chamber, under nitrogen protection in magnetic field strength be 2T's Oriented moulding in magnetic field, briquetting pressure 90MPa obtain pressing under magnetic field green compact；
(5) isostatic cool pressing
Pressing under magnetic field green compact obtained by step (4) are subjected to isostatic cool pressing, the pressure of isostatic cool pressing is 240MPa, isostatic cool pressing Time is 200s, and isostatic cool pressing green compact are obtained after release；
(6) low pressure sintering
Isostatic cool pressing green compact obtained by step (5) are put into low-pressure sintering furnace and close low-pressure sintering furnace and are vacuumized, When being evacuated to pressure≤1 × 10 in furnace-2It starts to warm up when Pa, when being warming up to 965 DEG C of heat preservation 1.0h, above-mentioned heating and kept the temperature Vacuum pumping is kept in journey, is stopped vacuumizing after heat preservation, is continued to the temperature in furnace at 965 DEG C and be passed through high-purity argon Pressure is that 2MPa heat-insulation pressure keeping is sintered 15min in gas to furnace, stops keeping the temperature and being passed through the progress of room temperature high-purity argon gas after sintering It is cooling, obtain sintered magnet；
(7) two-stage is heat-treated
Sintered magnet obtained by step (6) is heat-treated in low-pressure sintering furnace, operation is: discharge inert gas is laggard Row vacuumizes, when being evacuated to pressure≤1 × 10 in furnace-2It is started to warm up when Pa, 900 DEG C of heat preservation 2h is warming up to, after heat preservation Furnace cooling is to room temperature, then is warming up to 510 DEG C of heat preservation 4h, and furnace cooling arrives rare earth forever to room temperature after heat preservation Magnetic material keeps vacuum pumping during above-mentioned heating, heat preservation and furnace cooling.
Comparative example 10
Step (6) uses vacuum-sintering, remaining step is same as in Example 10.Vacuum sintering technology is 10-3~10- 2In 1060 DEG C of heat preservation sintering 4h under Pa vacuum condition, it is passed through room temperature high-purity argon gas after sintering and is cooled down, obtains sintering magnetic Body.
The rare earth permanent-magnetic material and embodiment 10 prepared with AMT-4 magnetization characteristic automatic measuring instrument difference test comparison example 10 The magnetic property of the magnetic property of the rare earth permanent-magnetic material of preparation, gained magnet is as follows:
Embodiment 11
The present embodiment prepares 25.57 (Pr, Nd) -7.13 (Ce, La) -65.11Fe-0.96B-0.71Al-0.52Cu rare earths Permanent-magnet material, processing step are as follows:
(1) ingredient
According to the chemical formula ingredient of above-mentioned rare earth permanent-magnetic material, and by the oxide on raw metal surface and to be mingled with removing dry Only；
(2) founding
The raw material that step (1) prepares is put into vacuum induction melting furnace, melting under the conditions of high-purity argon gas will close after melting Golden liquid casting on-line velocity is that the rapid hardening that average thickness is 0.25mm is obtained after being quickly cooled down on the water-cooled copper roller of 3m/s Alloy casting piece；
(3) magnetic powder is prepared
Alloy casting piece that step (2) obtains merging rotation hydrogen blasting furnace is subjected to suction hydrogen-Dehydroepiandrosterone derivative, obtain partial size be 10~ The rough and torn broken particle of gained alloy is carried out airflow milling under nitrogen protection and is crushed, is averaged by the rough and torn broken particle of 300 μm of alloy The mixing magnetic powder that partial size is 4.5 μm；
(4) pressing under magnetic field green compact are prepared
The antioxidant and lubricant (antioxygen of addition mixing magnetic powder quality 0.3wt% into mixing magnetic powder obtained by step (3) Agent and lubricant mass ratio 1:1), antioxidant is commercially available neodymium iron boron special antioxidant, and lubricant selects zinc stearate, Be uniformly mixed in batch mixer and form blank, then by blank embedded type chamber, under nitrogen protection in magnetic field strength be 1.8T Magnetic field in oriented moulding, briquetting pressure 50MPa obtains pressing under magnetic field green compact；
(5) isostatic cool pressing
Pressing under magnetic field green compact obtained by step (4) are subjected to isostatic cool pressing, the pressure of isostatic cool pressing is 200MPa, isostatic cool pressing Time is 200s, and isostatic cool pressing green compact are obtained after release；
(6) low pressure sintering
Isostatic cool pressing green compact obtained by step (5) are put into low-pressure sintering furnace and close low-pressure sintering furnace and are vacuumized, When being evacuated to pressure≤1 × 10 in furnace-2It starts to warm up when Pa, when being warming up to 960 DEG C of heat preservation 1.0h, above-mentioned heating and kept the temperature Vacuum pumping is kept in journey, is stopped vacuumizing after heat preservation, is continued to the temperature in furnace at 960 DEG C and be passed through high-purity argon Pressure is that 2MPa heat-insulation pressure keeping is sintered 25min in gas to furnace, stops keeping the temperature and being passed through the progress of room temperature high-purity argon gas after sintering It is cooling, obtain sintered magnet；
(7) two-stage is heat-treated
Sintered magnet obtained by step (6) is heat-treated in low-pressure sintering furnace, operation is: discharge inert gas is laggard Row vacuumizes, when being evacuated to pressure≤1 × 10 in furnace-2It is started to warm up when Pa, is warming up to 890 DEG C of heat preservation 1.5h, heat preservation terminates Furnace cooling is to room temperature afterwards, then is warming up to 505 DEG C of heat preservation 4h, and furnace cooling arrives rare earth to room temperature after heat preservation Permanent-magnet material keeps vacuum pumping during above-mentioned heating, heat preservation and furnace cooling.
Comparative example 11
Step (6) uses vacuum-sintering, remaining step is identical as embodiment 11.Vacuum sintering technology is 10-3~10- 2In 1060 DEG C of heat preservation sintering 4h under Pa vacuum condition, it is passed through room temperature high-purity argon gas after sintering and is cooled down, obtains sintering magnetic Body.
The rare earth permanent-magnetic material and embodiment 11 prepared with AMT-4 magnetization characteristic automatic measuring instrument difference test comparison example 11 The magnetic property of the magnetic property of the rare earth permanent-magnetic material of preparation, gained magnet is as follows:
Embodiment 12
The present embodiment prepares 24.29 (Nd, Pr) -8.03Ce-66.09Fe-0.99B-0.6TmRare earth permanent-magnetic material, technique Steps are as follows:
(1) ingredient
When ingredient, ingredient, the component of master alloying and the quality proportioning of component are first carried out respectively according to master alloying and auxiliary alloy For 28.58 (Nd0.8Pr0.2) -69.98Fe-1.02B-0.42Al, the component of auxiliary alloy and the quality proportioning of component are 53.49Ce- 44.06Fe-1.62Cu-0.83B, and by the oxide on raw metal surface and it is mingled with removing completely；
(2) founding
The raw material of master alloying and auxiliary alloy that step (1) prepares is respectively put into vacuum induction melting furnace, in high-purity argon gas Under the conditions of melting, after melting by aluminium alloy casting on-line velocity be 3m/s water-cooled copper roller on, obtained after being quickly cooled down The rapid hardening master alloying slab and auxiliary alloy casting piece that average thickness is 0.25mm；
(3) magnetic powder is prepared
Master alloying slab that step (2) obtains and auxiliary alloy casting piece are weighed according to mass ratio 85:15, will be weighed Master alloying slab and auxiliary alloy casting piece be placed in together rotation hydrogen blasting furnace in, carry out suction hydrogen-Dehydroepiandrosterone derivative, obtain partial size be 10~ The rough and torn broken particle of gained alloy is carried out airflow milling under nitrogen protection and is crushed, is averaged by the rough and torn broken particle of 300 μm of alloy The mixing magnetic powder that partial size is 4 μm；
(4) pressing under magnetic field green compact are prepared
Into mixing magnetic powder obtained by step (3), the antioxidant of addition mixing magnetic powder quality 0.25wt% and lubricant are (anti- Oxidant and lubricant mass ratio 1:1), antioxidant is commercially available neodymium iron boron special antioxidant, and lubricant selects zinc stearate, Be uniformly mixed in batch mixer and form blank, then by blank embedded type chamber, under nitrogen protection in magnetic field strength be 2T Magnetic field in oriented moulding, briquetting pressure 60MPa obtains pressing under magnetic field green compact；
(5) isostatic cool pressing
Pressing under magnetic field green compact obtained by step (4) are subjected to isostatic cool pressing, the pressure of isostatic cool pressing is 200MPa, isostatic cool pressing Time is 100s, and isostatic cool pressing green compact are obtained after release；
(6) low pressure sintering
Isostatic cool pressing green compact obtained by step (5) are put into low-pressure sintering furnace and close low-pressure sintering furnace and are vacuumized, When being evacuated to pressure≤1 × 10 in furnace-2It is started to warm up when Pa, when being warming up to 1000 DEG C of heat preservation 1.0h, above-mentioned heating and heat preservation Vacuum pumping is kept in the process, is stopped vacuumizing after heat preservation, is continued to the temperature in furnace at 1000 DEG C and be passed through height Pressure is that 2MPa heat-insulation pressure keeping is sintered 25min in pure argon to furnace, stops keeping the temperature after sintering and is passed through room temperature high-purity argon gas It is cooled down, obtains sintered magnet；
(7) two-stage is heat-treated
Sintered magnet obtained by step (6) is heat-treated in low-pressure sintering furnace, operation is: discharge inert gas is laggard Row vacuumizes, when being evacuated to pressure≤1 × 10 in furnace-2It is started to warm up when Pa, 905 DEG C of heat preservation 2h is warming up to, after heat preservation Furnace cooling is to room temperature, then is warming up to 550 DEG C of heat preservation 2h, and furnace cooling arrives rare earth forever to room temperature after heat preservation Magnetic material keeps vacuum pumping during above-mentioned heating, heat preservation and furnace cooling.
Comparative example 12
Step (6) is sintered using traditional vacuum, remaining step is identical as embodiment 12.Vacuum sintering technology is 10-3~ 10-2In 1040 DEG C of heat preservation sintering 4h under Pa vacuum condition, it is passed through room temperature high-purity argon gas after sintering and is cooled down, is sintered Magnet.
The rare earth permanent-magnetic material and embodiment 12 prepared with AMT-4 magnetization characteristic automatic measuring instrument difference test comparison example 12 The magnetic property of the magnetic property of the rare earth permanent-magnetic material of preparation, gained magnet is as follows:
Embodiment 13
The present embodiment prepares 24.96 (Nd, Pr) -7.71 (La, Ce) -65.14Fe-0.96B-1.23TmRare earth permanent magnet material Material, processing step are as follows:
(1) ingredient
When ingredient, ingredient, the component of master alloying and the quality proportioning of component are first carried out respectively according to master alloying and auxiliary alloy For 27.57 (Nd0.8Pr0.2) -70.69Fe-1.02B-0.72Al, the component of auxiliary alloy and the quality proportioning of component are 61.6MM- 33.7Fe-4.1Cu-0.6B (MM is mischmetal, mass ratio of each component 53.93%Ce, 29.35%La, 12.01%Nd, 4.71%Pr), and by the oxide on raw metal surface and it is mingled with removing completely；
(2) founding
The raw material of master alloying and auxiliary alloy that step (1) prepares is respectively put into vacuum induction melting furnace, in high-purity argon gas Under the conditions of melting, after melting by aluminium alloy casting on-line velocity be 3m/s water-cooled copper roller on, obtained after being quickly cooled down The rapid hardening master alloying slab and auxiliary alloy casting piece that average thickness is 0.25mm；
(3) magnetic powder is prepared
Master alloying slab that step (2) obtains and auxiliary alloy casting piece are weighed according to mass ratio 85:15, will be weighed Master alloying slab and auxiliary alloy casting piece be placed in together rotation hydrogen blasting furnace in, carry out suction hydrogen-Dehydroepiandrosterone derivative, obtain partial size be 10~ The rough and torn broken particle of gained alloy is carried out airflow milling under nitrogen protection and is crushed, is averaged by the rough and torn broken particle of 300 μm of alloy The mixing magnetic powder that partial size is 5.5 μm；
(4) pressing under magnetic field green compact are prepared
Into mixing magnetic powder obtained by step (3), the antioxidant of addition mixing magnetic powder quality 0.25wt% and lubricant are (anti- Oxidant and lubricant mass ratio 1:1), antioxidant is commercially available neodymium iron boron special antioxidant, and lubricant selects zinc stearate, Be uniformly mixed in batch mixer and form blank, then by blank embedded type chamber, under nitrogen protection in magnetic field strength be 2T Magnetic field in oriented moulding, briquetting pressure 50MPa obtains pressing under magnetic field green compact；
(5) isostatic cool pressing
Pressing under magnetic field green compact obtained by step (4) are subjected to isostatic cool pressing, the pressure of isostatic cool pressing is 200MPa, isostatic cool pressing Time is 120s, and isostatic cool pressing green compact are obtained after release；
(6) low pressure sintering
Isostatic cool pressing green compact obtained by step (5) are put into low-pressure sintering furnace and close low-pressure sintering furnace and are vacuumized, When being evacuated to pressure≤1 × 10 in furnace-2It is started to warm up when Pa, when being warming up to 1000 DEG C of heat preservation 1.0h, above-mentioned heating and heat preservation Vacuum pumping is kept in the process, is stopped vacuumizing after heat preservation, is continued to the temperature in furnace at 1000 DEG C and be passed through height Pressure is that 2MPa heat-insulation pressure keeping is sintered 25min in pure argon to furnace, stops keeping the temperature after sintering and is passed through room temperature high-purity argon gas It is cooled down, obtains sintered magnet；
(7) two-stage is heat-treated
Sintered magnet obtained by step (6) is heat-treated in low-pressure sintering furnace, operation is: discharge inert gas is laggard Row vacuumizes, when being evacuated to pressure≤1 × 10 in furnace-2It is started to warm up when Pa, 900 DEG C of heat preservation 2h is warming up to, after heat preservation Furnace cooling is to room temperature, then is warming up to 520 DEG C of heat preservation 2h, and furnace cooling arrives rare earth forever to room temperature after heat preservation Magnetic material keeps vacuum pumping during above-mentioned heating, heat preservation and furnace cooling.
Comparative example 13
The rare earth permanent-magnetic material and embodiment 13 prepared with AMT-4 magnetization characteristic automatic measuring instrument difference test comparison example 13 The magnetic property of the magnetic property of the rare earth permanent-magnetic material of preparation, gained magnet is as follows:

Claims (4)

1. a kind of preparation method of high-performance Ne-Fe-B rare earth permanent-magnetic material, it is characterised in that processing step is as follows:
(1) ingredient
Ingredient: RE 27%~34.5% is carried out according to the component of following rare earth permanent-magnetic material and the mass percentage of each component, Fe 61.5%~71%, B 0.9%~1.1%, Tm 0.1%~7%；The RE is at least one in Nd and Pr, Ce, La Kind, the Tm is at least one of Co, Cu, Al, Ga, Nb；
(2) founding
The raw material prepared in step (1) progress founding is obtained into alloy casting piece；
(3) magnetic powder is prepared
The alloy casting piece that step (2) obtains is subjected to suction hydrogen-Dehydroepiandrosterone derivative, it is rough and torn to obtain the alloy that partial size is 10 μm~300 μm The rough and torn broken particle of gained alloy is carried out airflow milling under inert gas protection and is crushed by broken particle, obtain average grain diameter be 3 μm~ 5 μm of mixing magnetic powder；
(4) pressing under magnetic field green compact are prepared
Antioxidant and lubricant are added into mixing magnetic powder obtained by step (3) and is uniformly mixed and forms blank, then by blank In embedded type chamber, the oriented moulding in magnetic field, obtains pressing under magnetic field green compact under inert gas protection；
(5) isostatic cool pressing
Pressing under magnetic field green compact obtained by step (4) are subjected to isostatic cool pressing, the pressure of isostatic cool pressing is 120MPa~320MPa, time For 10s~300s, isostatic cool pressing green compact are obtained after release；
(6) low pressure sintering
Isostatic cool pressing green compact obtained by step (5) are put into low-pressure sintering furnace and close low-pressure sintering furnace and are vacuumized, pumping is worked as Pressure≤1 × 10 in vacuum to furnace-2It is started to warm up when Pa, when being warming up to 900 DEG C~1000 DEG C heat preservation 0.5h~1.0h, above-mentioned liter Keep vacuum pumping in mild insulating process, stop vacuumizing after heat preservation, continue to temperature in furnace 900 DEG C~ 1000 DEG C and to be passed through in high purity inert gas to furnace pressure be that 0.5MPa~2MPa heat-insulation pressure keeping is sintered 5min~30min, sintering After stop keeping the temperature and be passed through room temperature high purity inert gas and be cooled to room temperature to obtain sintered magnet；
(7) two-stage is heat-treated
Sintered magnet obtained by step (6) is heat-treated, operation is in low-pressure sintering furnace: being taken out after discharge inert gas Vacuum, when being evacuated to pressure≤1 × 10 in furnace-2It is started to warm up when Pa, is warming up to 800 DEG C~950 DEG C heat preservation 0.5h~4h, protected Furnace cooling is to room temperature after temperature, then is warming up to 460 DEG C~600 DEG C heat preservation 1h~6h, and furnace cooling after heat preservation To room temperature to get rare earth permanent-magnetic material is arrived, vacuum pumping is kept during above-mentioned heating, heat preservation and furnace cooling.
2. the preparation method of high-performance Ne-Fe-B rare earth permanent-magnetic material according to claim 1, it is characterised in that described high-purity Inert gas is the nitrogen or argon gas of purity >=99.999%.
3. the preparation method of high-performance Ne-Fe-B rare earth permanent-magnetic material according to claim 1 or claim 2, it is characterised in that step (4) total addition level of antioxidant described in and lubricant is mix magnetic powder quality 0.05%~0.5%, antioxidant and profit The mass ratio of lubrication prescription is 1:1；Formed pressing under magnetic field green compact magnetic field strength be 1.5T~3T, briquetting pressure be 40MPa~ 100MPa。
4. the high-performance Ne-Fe-B rare earth permanent-magnetic material that in claims 1 to 3 prepared by any claim the method.
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